论文部分内容阅读
为提高花生中黄曲霉毒素B_1的检测效率和准确性,试验通过对提取溶剂、色谱条件和质谱条件的优化,建立了免疫亲和柱-超高效液相色谱串联质谱(UPLC-MS/MS)快速测定花生中黄曲霉毒素B_1的方法,并对方法进行了评估。结果表明,用甲醇-水(60∶40,V/V)对样品进行提取,采用黄曲霉毒素免疫亲和柱萃取、净化,以0.1%甲酸水溶液、0.1%甲酸乙腈溶液作为超高效液相色谱的流动相,在电喷雾离子源(ESI)正离子模式下采用多反应监测(MRM)对花生中黄曲霉毒素B_1进行定性、定量检测,在5.5 min内完成一个样品的分析。结果表明,黄曲霉毒素B_1在0.1~56.0 ng/m L的线性定量范围,相关系数高达0.999 42,检出限低至0.02μg/kg,定量限精确至0.1μg/kg,低、中、高浓度回收率为82%~92%,相对标准偏差<5%。该方法具有前处理简单、净化效果好和准确度高的优点,适用于花生等复杂基质样品的黄曲霉毒素B_1定性和定量检测。
In order to improve the detection efficiency and accuracy of aflatoxin B 1 in peanut, an immunoaffinity column-ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS / MS) was developed by optimizing extraction solvent, chromatographic conditions and mass spectrometry conditions. A rapid method for the determination of aflatoxin B1 in peanut and the method was evaluated. The results showed that the sample was extracted with methanol-water (60:40, V / V) and extracted with aflatoxin immunoaffinity column. The purified product was purified with 0.1% formic acid in water and 0.1% formic acid in acetonitrile as ultra performance liquid chromatography , The aflatoxin B 1 in peanut was qualitatively and quantitatively detected by multiple reaction monitoring (MRM) in electrospray ionization (ESI) positive ion mode, and a sample analysis was completed within 5.5 min. The results showed that the linearity range of aflatoxin B_1 was 0.1 ~ 56.0 ng / m L, the correlation coefficient was as high as 0.999 42, the detection limit was as low as 0.02 μg / kg, the limit of quantification was 0.1 μg / kg, the low, middle and high Concentration recovery rate of 82% to 92%, the relative standard deviation of <5%. The method has the advantages of simple pretreatment, good purification effect and high accuracy, and is suitable for the qualitative and quantitative determination of aflatoxin B 1 in complex matrix samples such as peanut.